関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-(Trifluoromethyl)pyrrolidine | HCID 5152159 | — |
| 反応物 | 2-[1-(2-Fluorobenzyl)-1H-pyrazolo[3,4-b]pyridin-3-yl]-4-iodo-5,5-dimethyl-5,7-dihydro-6H-pyrrolo[2,3-d]pyrimidin-6-one | HCID 86705367 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | HCID 71285706 | HCID 71285706 | — |
反応手順
Under an argon atmosphere, 200 mg (purity 62%, 0.24 mmol) of 2-[1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridin-3-yl]-4-iodo-5,5-dimethyl-5,7-dihydro-6H-pyrrolo[2,3-d]pyrimidin-6-one (example 15A) was put in 4 ml of absolute NMP and 671 mg (4.82 mmol) of 3-(trifluoromethyl)pyrrolidine was added. The mixture was heated in the microwave at 150° C. for 5 h. The reaction solution was filtered and purified by preparative HPLC (eluent: acetonitrile/water with 0.1% formic acid, gradient 20:80→100:0). 65 mg (49% of theor.) of the target compound was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08859569B2 |
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| 出典データセット | uspto-grants-2014_10 |
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| ORD ID | ord-1118da7cbd6149efb483f86ed714f2f3 |
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| 出典メモ | uspto-grants-2014_10 |
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